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CN102050424A - Method for preparing carbon nanotube thin film and method for preparing thin film transistor - Google Patents

Method for preparing carbon nanotube thin film and method for preparing thin film transistor Download PDF

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CN102050424A
CN102050424A CN2009101100468A CN200910110046A CN102050424A CN 102050424 A CN102050424 A CN 102050424A CN 2009101100468 A CN2009101100468 A CN 2009101100468A CN 200910110046 A CN200910110046 A CN 200910110046A CN 102050424 A CN102050424 A CN 102050424A
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carbon nano
tube film
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CN102050424B (en
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郑刚
李群庆
谢晶
范守善
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Tsinghua University
Hongfujin Precision Industry Shenzhen Co Ltd
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Hongfujin Precision Industry Shenzhen Co Ltd
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Abstract

The invention relates to a method for preparing a carbon nanotube thin film, which comprises the following steps of: providing a growth substrate on which a carbon nanotube array is formed; providing a first substrate, covering the first substrate on the carbon nanotube array and applying first pressure to the first substrate to press the carbon nanotube array so as to form a transition carbon nanotube film, wherein the adhesion of the first substrate and the transition carbon nanotube film is greater than that of the growth substrate and the transition carbon nanotube film; separating the first substrate from the growth substrate, and transferring the transition carbon nanotube film onto the surface of the first substrate; providing at least one second substrate, covering the second substrate on the surface of the transition carbon nanotube film, and applying second pressure to the second substrate; and separating the second substrate from the first substrate, transferring part of carbon nanotubes in the transition carbon nanotube film to the second substrate from the first substrate so as to prepare the carbon nanotube thin film on the surface of the second substrate.

Description

一种制备碳纳米管薄膜及薄膜晶体管的方法 A method for preparing carbon nanotube film and thin film transistor

技术领域technical field

本发明涉及一种制备薄膜及晶体管的方法，尤其涉及一种制备碳纳米管薄膜及薄膜晶体管的方法。The invention relates to a method for preparing a thin film and a transistor, in particular to a method for preparing a carbon nanotube thin film and a thin film transistor.

背景技术Background technique

硅电子器件是20世纪的重大发明之一。但是按照Moore定律(Moore定律是指IC上可容纳的晶体管数目，约每隔18个月便会增加一倍，性能也将提升一倍)，以硅材料为主的微电子到2011年的最小尺寸是0.08微米，达到物理极限，此后将是纳米电子学时代。Silicon electronics is one of the great inventions of the 20th century. However, according to Moore's law (Moore's law refers to the number of transistors that can be accommodated on an IC, which will double every 18 months, and the performance will also double), microelectronics based on silicon materials will be the smallest in 2011. The size is 0.08 microns, reaching the physical limit, after which it will be the era of nanoelectronics.

而碳纳米管以其优异的电学性质和机械性质，成为最有希望代替硅器件的下一代纳米电子器件。现有技术中通过化学气相沉积法可在硅基底上制备碳纳米管阵列，之后通过碾压处理该碳纳米管阵列可制得一碳纳米管碾压膜。然而这种碳纳米管碾压膜的厚度较大，用这种碾压膜一次制备某种器件时显得有些浪费，碳纳米管膜的利用率较低，进而使得器件成本较高，不适宜大规模生产。Carbon nanotubes have become the most promising next-generation nanoelectronic devices to replace silicon devices due to their excellent electrical and mechanical properties. In the prior art, a carbon nanotube array can be prepared on a silicon substrate by chemical vapor deposition, and then a carbon nanotube rolled film can be prepared by rolling the carbon nanotube array. However, the thickness of this carbon nanotube rolling film is relatively large, and it seems a bit wasteful to use this rolling film to prepare a certain device at one time. mass production.

发明内容Contents of the invention

有鉴于此，提供一种利用率较高、适合大规模生产的制备碳纳米管薄膜的方法实为必要。In view of this, it is necessary to provide a method for preparing carbon nanotube films with high utilization rate and suitable for large-scale production.

本发明涉及一种制备碳纳米管薄膜的方法，其包括以下步骤：提供一形成有碳纳米管阵列的生长基底；提供一第一基底，将该第一基底覆盖在碳纳米管阵列之上并施加一第一压力于该第一基底，从而使碳纳米管阵列被压形成一过渡碳纳米管膜，该第一基底与过渡碳纳米管膜的结合力比生长基底与过渡碳纳米管膜的结合力大；将该第一基底与生长基底分离，过渡碳纳米管膜被转印至第一基底的表面；提供至少一第二基底，将该第二基底覆盖在过渡碳纳米管膜的表面，施加一第二压力于该第二基底；将第二基底与第一基底分离，过渡碳纳米管膜中的部分碳纳米管由第一基底转印至第二基底，从而在第二基底的表面制得一碳纳米管薄膜。The invention relates to a method for preparing a carbon nanotube film, which comprises the following steps: providing a growth substrate formed with a carbon nanotube array; providing a first substrate, covering the first substrate on the carbon nanotube array and Applying a first pressure to the first substrate, so that the carbon nanotube array is pressed to form a transitional carbon nanotube film, the binding force between the first substrate and the transitional carbon nanotube film is greater than that of the growth substrate and the transitional carbon nanotube film The binding force is large; the first substrate is separated from the growth substrate, and the transition carbon nanotube film is transferred to the surface of the first substrate; at least one second substrate is provided, and the second substrate is covered on the surface of the transition carbon nanotube film , apply a second pressure on the second substrate; separate the second substrate from the first substrate, and transfer some of the carbon nanotubes in the transitional carbon nanotube film from the first substrate to the second substrate, so that A carbon nanotube film is prepared on the surface.

一种制备薄膜晶体管的方法，其包括以下步骤：提供基底和该基底表面形成的碳纳米管薄膜，该基底和碳纳米管薄膜是通过上述本发明的制备碳纳米管薄膜的方法制得的第二基底和形成于该第二基底表面上的碳纳米管薄膜；间隔形成一源极及一漏极于碳纳米管薄膜的表面，并使该源极及漏极与上述碳纳米管膜电连接；形成一绝缘层于上述碳纳米管膜表面；以及形成一栅极于上述绝缘层表面，得到一薄膜晶体管。A method for preparing a thin film transistor, which includes the following steps: providing a substrate and a carbon nanotube film formed on the surface of the substrate, the substrate and the carbon nanotube film are the first prepared by the method for preparing a carbon nanotube film of the present invention. Two substrates and a carbon nanotube film formed on the surface of the second substrate; forming a source electrode and a drain electrode on the surface of the carbon nanotube film at intervals, and electrically connecting the source electrode and the drain electrode to the above-mentioned carbon nanotube film ; forming an insulating layer on the surface of the carbon nanotube film; and forming a grid on the surface of the insulating layer to obtain a thin film transistor.

相对于现有技术，本发明提供的碳纳米管薄膜的制备方法过程简单，成本较低，一份碳纳米管阵列可以多次被转印，容易实现规模生产碳纳米管薄膜并适用于大面积制备薄膜晶体管等电子器件上，提高了碳纳米管阵列的利用率，相对的降低了制备薄膜晶体管等电子器件的成本。Compared with the prior art, the preparation method of the carbon nanotube film provided by the present invention is simple in process and low in cost. A carbon nanotube array can be transferred multiple times, and it is easy to realize large-scale production of the carbon nanotube film and is suitable for large-area In the preparation of electronic devices such as thin film transistors, the utilization rate of the carbon nanotube array is improved, and the cost of preparing electronic devices such as thin film transistors is relatively reduced.

附图说明Description of drawings

图1是本发明第一实施例提供的制备碳纳米管薄膜的方法的流程图。Fig. 1 is a flow chart of the method for preparing a carbon nanotube film provided by the first embodiment of the present invention.

图2至图7是本发明第一实施例提供的制备碳纳米管薄膜的方法各步骤的状态示意图。FIG. 2 to FIG. 7 are schematic diagrams of the states of each step of the method for preparing a carbon nanotube film provided by the first embodiment of the present invention.

图8是图3中碳纳米管阵列的倾倒方向的示意图。FIG. 8 is a schematic diagram of the pouring direction of the carbon nanotube array in FIG. 3 .

图9是本发明第一实施例提供的形成一相变聚合物材料层于所述过渡碳纳米管膜和第一基底之间的方法的流程图。Fig. 9 is a flow chart of the method for forming a phase-change polymer material layer between the transition carbon nanotube film and the first substrate according to the first embodiment of the present invention.

具体实施方式Detailed ways

为了对本发明作更进一步的说明，举以下具体实施例并配合附图详细描述如下。In order to further illustrate the present invention, the following specific embodiments are given and described in detail in conjunction with the accompanying drawings.

请参阅图1，本发明实施例提供一种制备碳纳米管薄膜的方法，其包括以下步骤：Please refer to Fig. 1, the embodiment of the present invention provides a kind of method for preparing carbon nanotube film, it comprises the following steps:

步骤S10，请参阅图2，提供一形成有碳纳米管阵列10的生长基底20。In step S10 , please refer to FIG. 2 , providing a growth substrate 20 on which the carbon nanotube array 10 is formed.

步骤S20，请参阅图3和图4，提供一第一基底30，将该第一基底30覆盖在碳纳米管阵列10之上并施加一第一压力于该第一基底30，从而使碳纳米管阵列10被压形成一过渡碳纳米管膜40。该第一基底30与过渡碳纳米管膜的结合力比生长基底20与过渡碳纳米管膜的结合力更大。Step S20, please refer to FIG. 3 and FIG. 4, provide a first substrate 30, cover the first substrate 30 on the carbon nanotube array 10 and apply a first pressure to the first substrate 30, so that the carbon nanotubes The tube array 10 is pressed to form a transitional carbon nanotube film 40 . The binding force between the first substrate 30 and the transitional carbon nanotube film is greater than the binding force between the growth substrate 20 and the transitional carbon nanotube film.

步骤S30，请参阅图5，将该第一基底30与生长基底20分离，过渡碳纳米管膜40被转移至第一基底30的表面。In step S30 , please refer to FIG. 5 , the first substrate 30 is separated from the growth substrate 20 , and the transition carbon nanotube film 40 is transferred to the surface of the first substrate 30 .

步骤S40，请参阅图6，提供一第二基底50，将该第二基底50覆盖在过渡碳纳米管膜40的表面，施加一第二压力于该第二基底50。In step S40 , please refer to FIG. 6 , a second substrate 50 is provided, the second substrate 50 is covered on the surface of the transition carbon nanotube film 40 , and a second pressure is applied to the second substrate 50 .

步骤S50，请参阅图7，将第二基底50与第一基底30分离，过渡碳纳米管膜40中的部分碳纳米管由第一基底30被转移至第二基底50，从而在第二基底50的表面制得一碳纳米管薄膜60。Step S50, please refer to FIG. 7, the second substrate 50 is separated from the first substrate 30, and part of the carbon nanotubes in the transition carbon nanotube film 40 are transferred from the first substrate 30 to the second substrate 50, so that A carbon nanotube film 60 is made on the surface of the 50.

在步骤S10中，所述碳纳米管阵列10包括多个垂直于所述生长基底20的碳纳米管。所述碳纳米管可以为单壁碳纳米管、双壁碳纳米管或多壁碳纳米管。所述碳纳米管阵列10可以位于生长基底20的全部表面或部分表面。本实施例中所述碳纳米管阵列10包括多个间隔设置且相互平行的条带状单壁碳纳米管阵列。所述每一条带状单壁碳纳米管阵列中多个碳纳米管之间具有一定的间隙。所述单壁碳纳米管阵列为多个彼此平行且垂直于生长基底20生长的碳纳米管形成的纯单壁碳纳米管阵列。In step S10 , the carbon nanotube array 10 includes a plurality of carbon nanotubes perpendicular to the growth substrate 20 . The carbon nanotubes may be single-wall carbon nanotubes, double-wall carbon nanotubes or multi-wall carbon nanotubes. The carbon nanotube array 10 may be located on the entire surface or part of the surface of the growth substrate 20 . The carbon nanotube array 10 in this embodiment includes a plurality of strip-shaped single-walled carbon nanotube arrays arranged at intervals and parallel to each other. There is a certain gap between the plurality of carbon nanotubes in each strip-shaped single-walled carbon nanotube array. The single-walled carbon nanotube array is a pure single-walled carbon nanotube array formed by a plurality of carbon nanotubes grown parallel to each other and perpendicular to the growth substrate 20 .

在步骤S20中，所述第一基底30的材料不限，只须满足第一基底30比生长基底20与碳纳米管有更大的结合力即可。具体地，第一基底30的材料包括聚对苯二甲酸乙二醇酯(PET)、聚二甲基硅氧烷(PDMS)、聚丙烯(PP)、聚氯乙烯(PVC)、聚乙烯(PE)、聚苯乙烯(PS)或聚对苯二甲酸丁二醇酯(PBT)。本实施例中，第一基底30的材料为PET。PET为柔性、透明材料且比硅基底与碳纳米管有更大的结合力。In step S20 , the material of the first substrate 30 is not limited, as long as the first substrate 30 has greater binding force with the carbon nanotubes than the growth substrate 20 . Specifically, the material of the first substrate 30 includes polyethylene terephthalate (PET), polydimethylsiloxane (PDMS), polypropylene (PP), polyvinyl chloride (PVC), polyethylene ( PE), polystyrene (PS) or polybutylene terephthalate (PBT). In this embodiment, the material of the first substrate 30 is PET. PET is a flexible, transparent material and has a greater bond to carbon nanotubes than silicon substrates.

所述第一压力应满足其具有一个平行于所述碳纳米管阵列10中碳纳米管的轴向且指向生长基底20的方向的分力。优选地，所述第一压力的方向可为平行于所述碳纳米管阵列10中碳纳米管的轴向且指向生长基底20的方向。The first pressure should satisfy that it has a component force parallel to the axial direction of the carbon nanotubes in the carbon nanotube array 10 and pointing to the growth substrate 20 . Preferably, the direction of the first pressure may be parallel to the axial direction of the carbon nanotubes in the carbon nanotube array 10 and point to the direction of the growth substrate 20 .

若第一压力的方向为平行于所述碳纳米管阵列10中碳纳米管的轴向且指向生长基底20的方向，则第一压力大于等于1兆帕，优选地为10-15兆帕。施加该第一压力的时间不少于5秒钟，优选地为不少于60秒。在该第一压力的作用下，该第一基底30将会压倒位于生长基底20之上的碳纳米管阵列10，从而使碳纳米管阵列10形成一过渡碳纳米管膜40，同时在该第一压力的作用下，过渡碳纳米管膜40与第一基底30较好的结合在一起。If the direction of the first pressure is parallel to the axial direction of the carbon nanotubes in the carbon nanotube array 10 and points to the growth substrate 20, the first pressure is greater than or equal to 1 MPa, preferably 10-15 MPa. The time for applying the first pressure is not less than 5 seconds, preferably not less than 60 seconds. Under the action of the first pressure, the first substrate 30 will overwhelm the carbon nanotube array 10 on the growth substrate 20, so that the carbon nanotube array 10 forms a transition carbon nanotube film 40, and at the same time Under the action of a certain pressure, the transitional carbon nanotube film 40 and the first substrate 30 are well bonded together.

本实施例中所述第一压力通过一压印机提供，所述压印机具有一光滑的压面，该压面提供一平行于所述碳纳米管阵列中碳纳米管的轴向的力而压倒碳纳米管阵列10。本实施例中，该第一压力的大小为12兆帕，施加该第一压力的时间为60秒。理论上而言，在该第一压力作用下碳纳米管阵列10中的碳纳米管可以沿任意方向倾倒。然而，若碳纳米管阵列10具有一定的形状，则碳纳米管阵列10中的碳纳米管优选地沿某一碳纳米管数量较少的方向倾倒，从而减小倾倒阻力。本实施例中，碳纳米管阵列包括多个条带状碳纳米管阵列。由于沿条带的长度方向生长有较多的碳纳米管，则碳纳米管在沿条带长度方向倾倒的过程中将承受较大的阻力。因此，碳纳米管优选的倾倒方向为沿条带的宽度方向。第一基底30同条带状碳纳米管阵列接触后，同时由于第一基底30同碳纳米管有较好的结合力，因此，在第一压力的作用下，条带状碳纳米管阵列的倾倒方向为沿条带的宽度方向的一侧倾倒。由于多个条带状碳纳米管阵列沿宽度之间存在一定距离的间隙，因此沿条带的宽度方向倾倒的碳纳米管会倾倒至条带之间的间隙处。同时，伴随着碳纳米管的倾倒，第一基底30同压面有一个相对的滑移。请参阅图8，其中b为一碳纳米管条带的宽度，a为一碳纳米管条带的长度。由图8中可以看出，碳纳米管条带沿宽度方向倾倒，相互间隔的碳纳米管条带之间存在一定的间隙，从而使碳纳米管倾倒于该间隙中。In this embodiment, the first pressure is provided by a stamping machine, the stamping machine has a smooth pressing surface, and the pressing surface provides a force parallel to the axial direction of the carbon nanotubes in the carbon nanotube array while overwhelming the carbon nanotube array 10 . In this embodiment, the magnitude of the first pressure is 12 MPa, and the time for applying the first pressure is 60 seconds. Theoretically, the carbon nanotubes in the carbon nanotube array 10 can fall in any direction under the action of the first pressure. However, if the carbon nanotube array 10 has a certain shape, the carbon nanotubes in the carbon nanotube array 10 are preferably toppled along a certain direction with fewer carbon nanotubes, so as to reduce the toppling resistance. In this embodiment, the carbon nanotube array includes a plurality of strip-shaped carbon nanotube arrays. Since more carbon nanotubes grow along the length direction of the strip, the carbon nanotubes will bear greater resistance during the process of falling along the length direction of the strip. Therefore, the preferred pouring direction of carbon nanotubes is along the width direction of the strip. After the first substrate 30 is in contact with the strip-shaped carbon nanotube array, at the same time because the first substrate 30 has a better bonding force with the carbon nanotube, therefore, under the effect of the first pressure, the strip-shaped carbon nanotube array The pouring direction is one side pouring along the width direction of the strip. Since there are gaps at a certain distance between the strip-shaped carbon nanotube arrays along the width, the carbon nanotubes falling along the width direction of the strips will fall to the gaps between the strips. At the same time, as the carbon nanotubes fall, the first substrate 30 has a relative slippage with the pressing surface. Please refer to FIG. 8 , where b is the width of a carbon nanotube strip, and a is the length of a carbon nanotube strip. It can be seen from FIG. 8 that the carbon nanotube strips are poured along the width direction, and there is a certain gap between the carbon nanotube strips spaced apart from each other, so that the carbon nanotubes are poured into the gap.

碳纳米管阵列倾倒后形成过渡碳纳米管膜40。过渡碳纳米管膜40的厚度为20-30微米，过渡碳纳米管膜40的厚度取决于碳纳米管条带的宽度b。过渡碳纳米管膜40中包括多个重叠的碳纳米管层。The transitional carbon nanotube film 40 is formed after the carbon nanotube array is poured. The thickness of the transitional carbon nanotube film 40 is 20-30 microns, and the thickness of the transitional carbon nanotube film 40 depends on the width b of the carbon nanotube strips. The transition carbon nanotube film 40 includes a plurality of overlapping carbon nanotube layers.

可选择地，在S10步骤之后S20步骤之前，于所述碳纳米管阵列10的自由端所形成的表面上可形成一相变聚合物材料层，之后提供第一基底30，并将第一基底30覆盖在碳纳米管阵列10的表面并施加第一压力，从而于过渡碳纳米管膜40和第一基底30之间形成一相变聚合物材料层。请参阅图9，所述形成一相变聚合物材料层于过渡碳纳米管膜40和第一基底30之间的方法具体包括以下步骤：Optionally, after step S10 and before step S20, a phase-change polymer material layer may be formed on the surface formed by the free ends of the carbon nanotube array 10, and then the first substrate 30 is provided, and the first substrate 30 covers the surface of the carbon nanotube array 10 and applies a first pressure to form a phase change polymer material layer between the transition carbon nanotube film 40 and the first substrate 30 . Please refer to FIG. 9, the method for forming a phase-change polymer material layer between the transition carbon nanotube film 40 and the first substrate 30 specifically includes the following steps:

步骤S201，提供一液态的相变聚合物材料，将该相变聚合物材料涂覆于碳纳米管阵列10的自由端所形成的表面上；Step S201, providing a liquid phase-change polymer material, and coating the phase-change polymer material on the surface formed by the free ends of the carbon nanotube array 10;

所述相变聚合物材料包括热固性材料或热塑性材料，具体地所述热固性材料包括聚二甲基硅氧烷(PDMS)，聚甲基丙烯酸甲酯(PMMA)或甲基丙烯酸甲酯(MMA)中的一种或多种。所述涂覆液态的相变聚合物材料的方法包括旋涂、涂刷、喷涂或浸涂。碳纳米管阵列中的碳纳米管之间存在一定间隙，相变聚合物材料会浸润至碳纳米管之间的间隙中。The phase change polymer material includes a thermosetting material or a thermoplastic material, specifically the thermosetting material includes polydimethylsiloxane (PDMS), polymethyl methacrylate (PMMA) or methyl methacrylate (MMA) one or more of. The method of coating the liquid phase change polymer material includes spin coating, brushing, spraying or dipping. There is a certain gap between the carbon nanotubes in the carbon nanotube array, and the phase change polymer material will infiltrate into the gap between the carbon nanotubes.

本实施例中，所述相变聚合物材料为PDMS，采用旋涂的方法将PDMS旋涂于多个条带状碳纳米管阵列的远离硅基底的自由端的表面。In this embodiment, the phase-change polymer material is PDMS, and the PDMS is spin-coated on the surfaces of the strip-shaped carbon nanotube arrays away from the free ends of the silicon substrate by using a spin-coating method.

步骤S202，提供所述第一基底30，将该第一基底30覆盖在碳纳米管阵列10的表面。Step S202 , providing the first substrate 30 and covering the surface of the carbon nanotube array 10 with the first substrate 30 .

步骤S203，施加一第一压力于该第一基底30的表面，同时或之后加热所述液态的相变聚合物材料使液态的相变聚合物材料固化形成相变聚合物材料层。在第一压力的作用下碳纳米管阵列10被压形成过渡碳纳米管膜40，且所述相变聚合物材料层形成于过渡碳纳米管膜40和第一基底30之间。Step S203 , applying a first pressure to the surface of the first substrate 30 , and simultaneously or subsequently heating the liquid phase change polymer material to solidify the liquid phase change polymer material to form a phase change polymer material layer. The carbon nanotube array 10 is pressed to form the transition carbon nanotube film 40 under the action of the first pressure, and the phase change polymer material layer is formed between the transition carbon nanotube film 40 and the first substrate 30 .

所述相变聚合物材料固化的温度和时间依据相变聚合物材料本身的性质而决定。由于相变聚合物材料浸润至碳纳米管阵列10之间的间隙中，因此相变聚合物材料层与过渡碳纳米管膜40和第一基底30较好地结合在一起。若相变聚合物材料为热固性材料，则该热固性材料的固化温度应低于第一基底30的玻璃化温度，从而保证在热固性材料的热固化过程中，第一基底30不会被破坏。若相变聚合物材料为热塑性材料，则该热塑性材料处于液态的温度应低于第一基底30的玻璃化温度，如此，当第一基底30和液态的热塑性材料接触时第一基底30不会被破坏。The curing temperature and time of the phase change polymer material are determined according to the properties of the phase change polymer material itself. Since the phase change polymer material infiltrates into the gaps between the carbon nanotube arrays 10 , the phase change polymer material layer is well combined with the transition carbon nanotube film 40 and the first substrate 30 . If the phase change polymer material is a thermosetting material, the curing temperature of the thermosetting material should be lower than the glass transition temperature of the first substrate 30, so as to ensure that the first substrate 30 will not be damaged during the thermal curing of the thermosetting material. If the phase-change polymer material is a thermoplastic material, the temperature of the thermoplastic material in a liquid state should be lower than the glass transition temperature of the first substrate 30, so that the first substrate 30 will not destroyed.

在步骤S30中，所述分离第一基底30与生长基底20的方法不限，只要可以将第一基底30与生长基底20分离且不破坏生长基底20表面的过渡碳纳米管膜40的结构即可。由于第一基底30同过渡碳纳米管膜40的结合力大于生长基底20同过渡碳纳米管膜40的结合力。因此，分离第一基底30和生长基底20之后，过渡碳纳米管膜40将会粘附在第一基底30的表面，从而使生长基底20表面的过渡碳纳米管膜40被转移到第一基底30的表面。本实施例中，采用镊子将第一基底30和生长基底20分离。In step S30, the method for separating the first substrate 30 and the growth substrate 20 is not limited, as long as the first substrate 30 and the growth substrate 20 can be separated without destroying the structure of the transition carbon nanotube film 40 on the surface of the growth substrate 20, that is, Can. Because the bonding force between the first substrate 30 and the transition carbon nanotube film 40 is greater than the bonding force between the growth substrate 20 and the transition carbon nanotube film 40 . Therefore, after separating the first substrate 30 and the growth substrate 20, the transition carbon nanotube film 40 will adhere to the surface of the first substrate 30, so that the transition carbon nanotube film 40 on the growth substrate 20 surface is transferred to the first substrate 30 surface. In this embodiment, tweezers are used to separate the first substrate 30 from the growth substrate 20 .

在步骤S40中，所述第二基底50的材料同第一基底30的材料可相同也可不同。所述第二基底50的材料包括聚对苯二甲酸乙二醇酯(PET)、聚二甲基硅氧烷(PDMS)、聚丙烯(PP)、聚氯乙烯(PVC)、聚乙烯(PE)、聚苯乙烯(PS)或聚对苯二甲酸丁二醇酯(PBT)中的一种或多种。本实施例中，第二基底50的材料同第一基底30的材料相同，为PET。In step S40 , the material of the second substrate 50 may be the same as or different from that of the first substrate 30 . The material of the second substrate 50 includes polyethylene terephthalate (PET), polydimethylsiloxane (PDMS), polypropylene (PP), polyvinyl chloride (PVC), polyethylene (PE ), polystyrene (PS) or polybutylene terephthalate (PBT). In this embodiment, the material of the second base 50 is the same as that of the first base 30 , which is PET.

若所述过渡碳纳米管膜40的表面形成有相变聚合物材料层，此时，由于过渡碳纳米管膜40通过所述相变聚合物材料层与第一基底30较好地结合在一起，因此在步骤S50中，过渡碳纳米管膜40中仅有较少的一部份碳纳米管被转印至第二基底50的表面。If a phase-change polymer material layer is formed on the surface of the transition carbon nanotube film 40, at this time, the transition carbon nanotube film 40 is better combined with the first substrate 30 through the phase-change polymer material layer. , so in step S50 , only a small part of the carbon nanotubes in the transitional carbon nanotube film 40 is transferred to the surface of the second substrate 50 .

若所述过渡碳纳米管膜40的表面没有形成相变聚合物材料层，则第二压力的大小应小于第一压力的大小，从而使小部分的过渡碳纳米管膜40中的碳纳米管由第一基底30转印至第二基底50。在步骤S20中，施加第一压力于第一基底30，从而使第一基底30表面的碳纳米管阵列10形成过渡碳纳米管膜40。该过渡碳纳米管膜40中包括多个碳纳米管层，且过渡碳纳米管膜40与第一基底30的结合力大于过渡碳纳米管膜40中各个碳纳米管层之间的结合力。各碳纳米管层之间的结合力随着与第一基底30的距离的增大而呈梯度减小。距离第一基底30越远的各碳纳米管层之间的结合力越小，距离第一基底30最远的两碳纳米管层之间的结合力最小。这是由于，过渡碳纳米管膜40中相邻两碳纳米管层之间的结合力为范德华力，其大小取决于相邻两碳纳米管层之间的范德华力的大小，以及相邻两碳纳米管层之间通过范德华力作用的接触面积。距离第一基底30越近，过渡碳纳米管膜40被压得越密实，相邻两碳纳米管层之间的接触面积越大，从而范德华力的有效作用面积也越大。另一方面，相邻两碳纳米管层之间的距离变小，从而使相邻两碳纳米管层之间的范德华力变大。在步骤S40中，施加第二压力于第二基底50，第二压力小于第一压力。此时，过渡碳纳米管膜40与第一基底30的结合力为一最大值F1，随着与第一基底30的距离的增加，各碳纳米管层之间结合力逐渐减小，并达到一最小值，之后，随着与第二基底50的距离的减小，碳纳米管层之间的结合力逐渐增加，过渡碳纳米管膜40与第二基底50的结合力达到一个较大值F2，且F2＜F1。因此，在分离第二基底50与第一基底30时，过渡碳纳米管膜40从相互作用的结合力最小的两个碳纳米管层之间分离。且由于第二压力小于第一压力，因此，该相互作用的结合力最小的两个碳纳米管层的位置距离第二基底50较近。从而在分离第二基底50和第一基底30之后过渡碳纳米管膜40中仅有少部分碳纳米管被转印至第一基底30表面。If no phase-change polymer material layer is formed on the surface of the transition carbon nanotube film 40, the second pressure should be smaller than the first pressure, so that the carbon nanotubes in a small portion of the transition carbon nanotube film 40 Transfer printing from the first substrate 30 to the second substrate 50 . In step S20 , a first pressure is applied to the first substrate 30 , so that the carbon nanotube array 10 on the surface of the first substrate 30 forms a transitional carbon nanotube film 40 . The transition carbon nanotube film 40 includes a plurality of carbon nanotube layers, and the bonding force between the transition carbon nanotube film 40 and the first substrate 30 is greater than the bonding force between the carbon nanotube layers in the transition carbon nanotube film 40 . The bonding force between the carbon nanotube layers decreases in a gradient as the distance from the first substrate 30 increases. The farther away from the first substrate 30 the bonding force between the carbon nanotube layers is smaller, and the bonding force between the two carbon nanotube layers farthest from the first substrate 30 is the smallest. This is because the bonding force between two adjacent carbon nanotube layers in the transition carbon nanotube film 40 is van der Waals force, and its size depends on the size of the van der Waals force between adjacent two carbon nanotube layers, and the strength of the two adjacent carbon nanotube layers. The contact area between carbon nanotube layers through van der Waals forces. The closer to the first substrate 30 , the denser the transitional carbon nanotube film 40 is pressed, the larger the contact area between two adjacent carbon nanotube layers, and thus the larger the effective area of van der Waals force. On the other hand, the distance between two adjacent carbon nanotube layers becomes smaller, so that the van der Waals force between two adjacent carbon nanotube layers becomes larger. In step S40, a second pressure is applied to the second substrate 50, and the second pressure is lower than the first pressure. At this time, the bonding force between the transitional carbon nanotube film 40 and the first substrate 30 is a maximum value F 1 , and as the distance from the first substrate 30 increases, the bonding force between the carbon nanotube layers gradually decreases, and Reach a minimum value, after that, as the distance from the second substrate 50 decreases, the binding force between the carbon nanotube layers gradually increases, and the binding force between the transition carbon nanotube film 40 and the second substrate 50 reaches a greater value F 2 , and F 2 <F 1 . Therefore, when the second substrate 50 is separated from the first substrate 30 , the transitional carbon nanotube film 40 is separated from between the two carbon nanotube layers with the smallest interaction binding force. And because the second pressure is lower than the first pressure, the positions of the two carbon nanotube layers with the smallest binding force of the interaction are closer to the second substrate 50 . Therefore, after the second substrate 50 and the first substrate 30 are separated, only a small part of the carbon nanotubes in the transitional carbon nanotube film 40 is transferred to the surface of the first substrate 30 .

所述第二压力的大小为大于等于1兆帕，优选地为3-8兆帕。所述施加第二压力的时间为不少于5秒钟，优选地为不少于60秒钟。由此可以使得在步骤S50中，所制得的碳纳米管薄膜60(最终成品膜)具有较薄的厚度。The magnitude of the second pressure is greater than or equal to 1 MPa, preferably 3-8 MPa. The time for applying the second pressure is not less than 5 seconds, preferably not less than 60 seconds. Thus, in step S50, the carbon nanotube thin film 60 (final finished film) produced has a thinner thickness.

在步骤S50，所述分离第二基底50与第一基底30的方法同步骤S30中分离第一基底30与形成有碳纳米管阵列10的生长基底20的方法相同。In step S50, the method of separating the second substrate 50 from the first substrate 30 is the same as the method of separating the first substrate 30 from the growth substrate 20 formed with the carbon nanotube array 10 in step S30.

本实施例中，第二基底50的表面制得的碳纳米管薄膜60的厚度大于等于10纳米。本实施例中，所制得的碳纳米管薄膜60的厚度为500-1000纳米。此时碳纳米管薄膜60仍位于PET的表面，由于PET为柔性、透明材料，因此该位于PET表面的碳纳米管薄膜60可被用于制备薄膜晶体管。In this embodiment, the thickness of the carbon nanotube film 60 formed on the surface of the second substrate 50 is greater than or equal to 10 nanometers. In this embodiment, the thickness of the prepared carbon nanotube film 60 is 500-1000 nanometers. At this time, the carbon nanotube film 60 is still located on the surface of the PET. Since PET is a flexible and transparent material, the carbon nanotube film 60 located on the surface of the PET can be used to prepare a thin film transistor.

可选择地，对该位于第二基底50表面的碳纳米管薄膜60进行清洗从而进一步降低碳纳米管薄膜60的厚度，同时还可使碳纳米管薄膜60的厚度均匀。通过清洗过程可以有效地控制碳纳米管薄膜60的厚度。本实施例中将所述碳纳米管薄膜60在丙酮溶液中超声处理10分钟，使碳纳米管薄膜60的厚度降低至50纳米。Optionally, the carbon nanotube film 60 located on the surface of the second substrate 50 is cleaned so as to further reduce the thickness of the carbon nanotube film 60 and also make the thickness of the carbon nanotube film 60 uniform. The thickness of the carbon nanotube film 60 can be effectively controlled through the cleaning process. In this embodiment, the carbon nanotube film 60 is ultrasonically treated in an acetone solution for 10 minutes to reduce the thickness of the carbon nanotube film 60 to 50 nanometers.

可选择地，可依次提供多个第二基底，并重复步骤S40和S50，多次将第一基底30表面的过渡碳纳米管膜40的一部分转印至第二基底上，从而制备多个碳纳米管薄膜。可以理解的是，伴随着依次提供多个第二基底，因为越靠近第一基底的碳纳米管层之间的结合力越大，所以相应的依次施加于靠后的第二基底上的力也逐渐增加，从而确保有分离第二基底和第一基底之后有部分碳纳米管被转印至第二基底的表面。Alternatively, a plurality of second substrates may be provided sequentially, and steps S40 and S50 are repeated to transfer a part of the transition carbon nanotube film 40 on the surface of the first substrate 30 to the second substrate multiple times, thereby preparing a plurality of carbon nanotubes. nanotube film. It can be understood that, as a plurality of second substrates are sequentially provided, since the bonding force between the carbon nanotube layers closer to the first substrate is greater, the corresponding force sequentially applied to the rear second substrates is also gradually increased to ensure that some carbon nanotubes are transferred to the surface of the second substrate after separating the second substrate from the first substrate.

可选择地，可提供一大面积的第二基底，并重复步骤S40和S50，多次将第一基底30表面的过渡碳纳米管膜40的一部分转印至第二基底的不同区域，从而得到一大面积碳纳米管薄膜，进而可用于大面积制备薄膜晶体管等电子器件。Alternatively, a large-area second substrate can be provided, and steps S40 and S50 are repeated to transfer a part of the transition carbon nanotube film 40 on the surface of the first substrate 30 to different regions of the second substrate multiple times, thereby obtaining A large-area carbon nanotube film can be used to prepare electronic devices such as thin-film transistors in a large area.

本发明提供的碳纳米管薄膜的制备方法过程简单，成本较低，一份碳纳米管阵列可以多次被转印，容易实现规模生产碳纳米管薄膜并适用于大面积制备薄膜晶体管等电子器件上，提高了碳纳米管阵列的利用率，相对的降低制备薄膜晶体管等电子器件的成本。The preparation method of the carbon nanotube film provided by the present invention is simple in process and low in cost, and a carbon nanotube array can be transferred multiple times, and it is easy to realize large-scale production of the carbon nanotube film and is suitable for large-area preparation of electronic devices such as thin film transistors Above all, the utilization rate of the carbon nanotube array is improved, and the cost of preparing electronic devices such as thin film transistors is relatively reduced.

一种制备薄膜晶体管的方法，其包括以下步骤：A method for preparing a thin film transistor, comprising the steps of:

步骤S12，提供一表面形成有碳纳米管薄膜60的第二基底50，该第二基底50上的碳纳米管薄膜60是通过上述本发明实施例的转印方法制得；Step S12, providing a second substrate 50 with a carbon nanotube film 60 formed on its surface, the carbon nanotube film 60 on the second substrate 50 is produced by the transfer method of the above-mentioned embodiment of the present invention;

步骤S22，间隔形成一源极及一漏极于碳纳米管薄膜60的表面，并使该源极及漏极与上述碳纳米管薄膜60电连接；Step S22, forming a source electrode and a drain electrode on the surface of the carbon nanotube film 60 at intervals, and electrically connecting the source electrode and the drain electrode to the carbon nanotube film 60;

步骤S32，形成一绝缘层于上述碳纳米管薄膜60表面；Step S32, forming an insulating layer on the surface of the carbon nanotube film 60;

步骤S42，以及形成一栅极于上述绝缘层表面，得到一薄膜晶体管。Step S42, and forming a gate on the surface of the insulating layer to obtain a thin film transistor.

在步骤S12中，碳纳米管薄膜60中的碳纳米管都是平行排列，处于并联状态，因此工作状态稳定。碳纳米管薄膜60中的碳纳米管为单壁碳纳米管，因此，该碳纳米管薄膜60为半导体性，其可作为薄膜晶体管的半导体层。In step S12, the carbon nanotubes in the carbon nanotube film 60 are all arranged in parallel and are in a parallel state, so the working state is stable. The carbon nanotubes in the carbon nanotube film 60 are single-walled carbon nanotubes. Therefore, the carbon nanotube film 60 is semiconducting and can be used as a semiconductor layer of a thin film transistor.

在步骤S22中，该源极及漏极的材料应具有较好的导电性。具体地，该源极及漏极的材料可以为金属、合金、铟锡氧化物(ITO)、锑锡氧化物(ATO)、导电银胶、导电聚合物以及金属性碳纳米管等导电材料。根据形成源极及漏极的材料种类的不同，可以采用不同方法形成该源极及漏极。具体地，当该源极及漏极的材料为金属、合金、ITO或ATO时，可以通过蒸镀、溅射、沉积、掩模及刻蚀等方法形成源极及漏极。当该源极及漏极的材料为导电银胶、导电聚合物或金属性碳纳米管时，可以通过印刷涂附或直接黏附的方法，将该导电银胶或金属性碳纳米管涂附或黏附于绝缘基底或碳纳米管层表面，形成源极及漏极。一般地，该源极及漏极的厚度为0.5纳米～100微米，源极和漏极之间的距离为1～100微米。In step S22, the material of the source and the drain should have better conductivity. Specifically, the material of the source electrode and the drain electrode can be conductive materials such as metal, alloy, indium tin oxide (ITO), antimony tin oxide (ATO), conductive silver paste, conductive polymer, and metallic carbon nanotubes. According to different types of materials forming the source and drain, different methods can be used to form the source and drain. Specifically, when the material of the source and drain is metal, alloy, ITO or ATO, the source and drain can be formed by methods such as evaporation, sputtering, deposition, masking and etching. When the source and drain materials are conductive silver glue, conductive polymer or metallic carbon nanotubes, the conductive silver glue or metallic carbon nanotubes can be coated or coated by printing or direct adhesion. Adhere to the insulating substrate or the surface of the carbon nanotube layer to form the source and drain. Generally, the thickness of the source and the drain is 0.5 nanometers to 100 microns, and the distance between the source and the drain is 1 to 100 microns.

在步骤S32，所述绝缘层的材料为氮化硅、氧化硅等硬性材料或苯并环丁烯(BCB)、聚酯或丙烯酸树脂等柔性材料。该绝缘层的厚度为5纳米-100微米。本实施例中，所述绝缘层的材料为氮化硅。可以理解，根据具体的形成工艺不同，所述绝缘层不必完全覆盖所述源极、漏极及半导体层，只要能保证半导体层、源极和漏极与其相对设置的栅极绝缘即可。In step S32, the insulating layer is made of hard materials such as silicon nitride and silicon oxide or flexible materials such as benzocyclobutene (BCB), polyester or acrylic resin. The insulating layer has a thickness of 5 nanometers to 100 micrometers. In this embodiment, the material of the insulating layer is silicon nitride. It can be understood that, depending on the specific formation process, the insulating layer does not have to completely cover the source, drain and semiconductor layer, as long as the semiconductor layer, source and drain are insulated from the gate opposite to them.

在步骤S42，该栅极120的材料应具有较好的导电性。具体地，该栅极的材料可以为金属、合金、ITO、ATO、导电银胶、导电聚合物以及碳纳米管薄膜等导电材料。该金属或合金材料可以为铝、铜、钨、钼、金或它们的合金。具体地，当该栅极120的材料为金属、合金、ITO或ATO时，可以通过蒸镀、溅射、沉积、掩模及刻蚀等方法形成栅极。当该栅极的材料为导电银胶、导电聚合物或碳纳米管薄膜时，可以通过直接黏附或印刷涂附的方法形成栅极。一般地，该栅极的厚度为0.5纳米～100微米。In step S42, the material of the gate 120 should have better conductivity. Specifically, the material of the gate can be conductive materials such as metal, alloy, ITO, ATO, conductive silver paste, conductive polymer, and carbon nanotube film. The metal or alloy material can be aluminum, copper, tungsten, molybdenum, gold or their alloys. Specifically, when the material of the gate 120 is metal, alloy, ITO or ATO, the gate can be formed by methods such as evaporation, sputtering, deposition, masking and etching. When the material of the grid is conductive silver glue, conductive polymer or carbon nanotube film, the grid can be formed by direct adhesion or printing coating. Generally, the gate has a thickness of 0.5 nanometers to 100 micrometers.

本发明提供的采用碳纳米管薄膜制备薄膜晶体管的方法过程简单，成本很低，过程可以重复，适用于大面积制备薄膜晶体管，可以用于工业生产。The method for preparing a thin film transistor by using a carbon nanotube thin film provided by the invention has simple process, low cost and repeatable process, is suitable for preparing a thin film transistor in a large area, and can be used in industrial production.

Claims (21)

1. method for preparing carbon nano-tube film, it may further comprise the steps:
One growth substrate that is formed with carbon nano pipe array is provided;
One first substrate is provided, cover this first substrate on the carbon nano pipe array and apply one first pressure in this first substrate, thereby carbon nano pipe array is pressed form a transition carbon nano-tube film, this first substrate is bigger than the adhesion of growth substrate and transition carbon nano-tube film with the adhesion of transition carbon nano-tube film;
This first substrate is separated with growth substrate, and the transition carbon nano-tube film is transferred to the surface of first substrate;
At least one second substrate is provided, this second substrate is covered the surface of transition carbon nano-tube film, apply one second pressure in this second substrate;
Second substrate is separated with first substrate, and the part CNT in the transition carbon nano-tube film is transferred to second substrate by first substrate, thereby makes a carbon nano-tube film on the surface of second substrate.
2. the method for preparing carbon nano-tube film as claimed in claim 1 is characterized in that, a plurality of second substrates are provided successively, and successively the part CNT in the transition carbon nano-tube film is transferred to second substrate surface, thereby obtains a plurality of carbon nano-tube films.
3. the method for preparing carbon nano-tube film as claimed in claim 1 is characterized in that, the described size that puts on first pressure on first substrate is more than or equal to 1 MPa, and the time that applies this first pressure is more than or equal to 5 seconds.
4. the method for preparing carbon nano-tube film as claimed in claim 3 is characterized in that, the time that the described size that puts on first pressure on first substrate is the 10-15 MPa, apply this first pressure is for more than or equal to 60 seconds.
5. the method for preparing carbon nano-tube film as claimed in claim 1 is characterized in that, the size of described second pressure is more than or equal to 1 MPa, and the time that applies second pressure is more than or equal to 5 seconds.
6. the method for preparing carbon nano-tube film as claimed in claim 5 is characterized in that the size of described second pressure is the 3-8 MPa, and the time that applies second pressure is more than or equal to 60 seconds.
7. the method for preparing carbon nano-tube film as claimed in claim 1, it is characterized in that, describedly provide one to be formed with after the step of growth substrate of carbon nano pipe array, provide before the step of one first substrate, further may further comprise the steps: the phase transformation polymeric material that a liquid state is provided; This phase transformation polymeric material is coated on the surface of the free end formation of carbon nano pipe array.
8. the method for preparing carbon nano-tube film as claimed in claim 7, it is characterized in that, described phase transformation polymeric material comprises thermosets and thermoplastic, the heat curing temperature of this thermosets is lower than the vitrification point of first substrate, this thermoplastic be in liquid state the time temperature be lower than the vitrification point of first substrate.
9. the method for preparing carbon nano-tube film as claimed in claim 8 is characterized in that described thermosets comprises dimethyl silicone polymer, one or more in polymethyl methacrylate or the methyl methacrylate.
10. the method for preparing carbon nano-tube film as claimed in claim 8 is characterized in that, describedly applies one first pressure in the time of the step of this first substrate or afterwards, also draws together following steps: heat described thermosets described thermosets is solidified.
11., it is characterized in that described second pressure is less than first pressure as each described method for preparing carbon nano-tube film in the claim 1 to 10.
12. the method for preparing carbon nano-tube film as claimed in claim 1 is characterized in that, carbon nano pipe array comprises the ribbon carbon nano pipe array that a plurality of intervals are provided with and are parallel to each other.
13. the method for preparing carbon nano-tube film as claimed in claim 1, it is characterized in that, the material of described first substrate comprises one or more in PETG, dimethyl silicone polymer, polypropylene, polyvinyl chloride, polyethylene, polystyrene or the polybutylene terephthalate (PBT), and the material of described second substrate comprises one or more in PETG, dimethyl silicone polymer, polypropylene, polyvinyl chloride, polyethylene, polystyrene or the polybutylene terephthalate (PBT).
14. a method for preparing carbon nano-tube film, it may further comprise the steps:
One first substrate is provided, and this first substrate is provided with a transition carbon nano-tube film;
At least one second substrate is provided, and the adhesion of the CNT in this second substrate and the transition carbon nano-tube film is not more than the adhesion of the CNT in first substrate and the transition carbon nano-tube film;
This second substrate is covered the surface of transition carbon nano-tube film and applies a pressure in this second substrate and first substrate;
Second substrate is separated with first substrate, and the part CNT is transferred to second substrate by first substrate, thereby makes a carbon nano-tube film on the surface of second substrate.
15. the method for preparing carbon nano-tube film as claimed in claim 14 is characterized in that, the size of described pressure is more than or equal to 1 MPa, and the time of exerting pressure is more than or equal to 5 seconds.
16. the method for preparing carbon nano-tube film as claimed in claim 14 is characterized in that, forms a phase transformation polymer material layer between the described transition carbon nano-tube film and first substrate.
17. the method for preparing carbon nano-tube film as claimed in claim 14 is characterized in that, a plurality of second substrates are provided successively, and successively the part CNT in the transition carbon nano-tube film is transferred to second substrate surface, thereby obtains a plurality of carbon nano-tube films.
18. method for preparing thin film transistor (TFT), it may further comprise the steps: the carbon nano-tube film that provides a substrate and this substrate surface to form, described substrate and carbon nano-tube film serve as reasons second substrate that obtains as any described method in the claim 1 to 19 and the carbon nano-tube film that is formed on this second substrate surface; Form one source pole and at interval and drain, and this source electrode and drain electrode are electrically connected with above-mentioned carbon nano-tube film in the carbon nano-tube film surface; Form an insulating barrier in above-mentioned carbon nano-tube film surface; And form a grid in above-mentioned surface of insulating layer, obtain a thin film transistor (TFT).
19. the method for preparing thin film transistor (TFT) as claimed in claim 18 is characterized in that CNT is arranged in parallel in the described carbon nano-tube film, is in state in parallel.
20. the method for preparing thin film transistor (TFT) as claimed in claim 18 is characterized in that, the CNT in the described carbon nano-tube film is a SWCN.
21. the method for preparing thin film transistor (TFT) as claimed in claim 18, it is characterized in that described base material is one or more in PETG, dimethyl silicone polymer, polypropylene, polyvinyl chloride, polyethylene, polystyrene or the polybutylene terephthalate (PBT).
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